[1]章亚东,邢军伟..硫脲法合成1,2-乙二硫醇的后处理工艺研究[J].郑州大学学报(工学版),2009,30(02):23-26.[doi:10.3969/j.issn.1671-6833.2009.02.006]
　Zhang Yadong,Xing Junwei.Study on the post-treatment process of synthesis of 1,2-ethylenedithiol by thiourea method[J].Journal of Zhengzhou University (Engineering Science),2009,30(02):23-26.[doi:10.3969/j.issn.1671-6833.2009.02.006]

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硫脲法合成1,2-乙二硫醇的后处理工艺研究()

分享到：

《郑州大学学报(工学版)》[ISSN:1671-6833/CN:41-1339/T]

卷:

30卷

期数:

2009年02期

页码:

23-26

栏目:

出版日期:

1900-01-01

文章信息/Info

Title:

Study on the post-treatment process of synthesis of 1,2-ethylenedithiol by thiourea method

作者:

章亚东; 邢军伟.

郑州大学化工学院,河南,郑州,450001, 郑州大学化工学院,河南,郑州,450001

Author(s):

Zhang Yadong; Xing Junwei

关键词:

1;  2-乙二硫醇;  硫脲;  后处理;  回收

Keywords:

1;  2-Ethanedithiol;  thiourea;  post-processing;  Recycling

DOI:

10.3969/j.issn.1671-6833.2009.02.006

文献标志码:

A

摘要:

通过硫脲和S-烃基异硫脲盐在溶剂95%乙醇中溶解度的测定,确定了它们在最终反应液中的含量,减少了溶剂用量,省去了蒸馏回收乙醇的后处理操作步骤,使溶剂的循环利用率可达90%以上.根据Na2SO4和NaBr在水中溶解度的差异,通过旋转蒸发从反应液水相中分离出了Na2SO4和NaBr,Na2SO4的回收率可达95%以上.通过气质联用确定了油相的组成,采用减压蒸馏得到了纯度99%以上的产品,最终收率可达70%以上.釜液经过锌粉还原,得到了副产物二巯基二乙基硫醚.

Abstract:

Through the determination of the solubility of thiourea and S-hydrocarbon isothiourea salts in solvent 95% ethanol, their content in the final reaction solution was determined, the amount of solvent was reduced, the post-treatment operation step of distillation and ethanol recovery was eliminated, and the recycling rate of solvent could reach more than 90%. According to the difference in solubility of Na2SO4 and NaBr in water, Na2SO4 and NaBr were separated from the aqueous phase of the reaction liquid by rotary evaporation, and the recovery rate of Na2SO4 could reach more than 95%. The composition of the oil phase was determined by gas chromatography-mass spectrometry, and the product with a purity of more than 99% was obtained by vacuum distillation, and the final yield could reach more than 70%. The kettle liquid was reduced by zinc powder to obtain a by-product dimercaptodiethyl sulfide.

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